WO2005031299A2 - Plate-forme de detection utilisant a element nanotubulaire non horizontal - Google Patents
Plate-forme de detection utilisant a element nanotubulaire non horizontal Download PDFInfo
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- WO2005031299A2 WO2005031299A2 PCT/US2004/014999 US2004014999W WO2005031299A2 WO 2005031299 A2 WO2005031299 A2 WO 2005031299A2 US 2004014999 W US2004014999 W US 2004014999W WO 2005031299 A2 WO2005031299 A2 WO 2005031299A2
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- sensor element
- sensor
- nanotube
- collection
- conductive
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- G11C13/025—Digital stores characterised by the use of storage elements not covered by groups G11C11/00, G11C23/00, or G11C25/00 using elements whose operation depends upon chemical change using fullerenes, e.g. C60, or nanotubes, e.g. carbon or silicon nanotubes
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Definitions
- Nanotube Films and Articles (U.S. Pat. Appl. Ser. No. 10/128,118), filed April 23, 2002; Electromechanical Memory Array Using Nanotube Ribbons .and Method for Making Same (U.S. Pat. Appl. Ser. No. 09/915,093), filed on July 25, 2001; Electromechanical Three-Trace Junction Devices (U.S. Pat. Appl. Ser. No. 10/033,323), filed on December 28, 2001; Methods of Making Carbon Nanotube Films, Layers, Fabrics, Ribbons, Elements and Articles (U.S. Pat. Appl. Ser. No.
- the present application relates generally to methods for the detection of target analytes .and for measuring or detecting various electrical values by utilizing individual nanosensors and nanosensor arrays, and the application more particularly relates to means or platforms for creating such sensors .and sensor arrays.
- Chemical sensors made of nanotubes may be functionalized or otherwise modified to become molecule-specific or species-specific sensors, see P. Qi et .al., "Tow.ard Large Arrays of Multiplex Functionalized Carbon Nanotube Sensors for Highly Sensitive and Selective Molecular Detection," Nano Lett, vol. 3, no. 3, pp. 347-51 (2003); Dai et al., "Carbon Nanotube Sensing," U.S. Patent Appl. Ser. No. 10/175,026, filed on June 18, 2002.
- such sensors may comprise non-functionalized semiconducting tubes and may sense for the presence of known chemicals, see, e.g., Kong, supra.
- the invention relates to one or more sensor platforms and methods of making such platforms wherein sensor platforms include sensor elements oriented substantiality non-horizontally - e.g., subst.antially vertically - with respect to a major surface of a substrate (which is understood to be "horizontal").
- a sensor element comprises one or more nanostructures such as nanotubes.
- a sensor element may have or may be made to have an affinity for a corresponding analyte.
- a sensor platform includes a sensor element having a collection of nanotubes with one or more measurable electrical characteristics.
- a support structure supports the sensor element so that it may be exposed to a fluid, and control circuitry electrically senses the electrical characterization of the sensor element so that the presence of a corresponding analyte may be detected.
- a sensor element has an affinity for the corresponding analyte.
- nanotubes used are pristine nanotubes.
- nanotubes are derivatized to have or to increase the affinity.
- nanotubes are functionalized to have or to increase the affinity.
- the sensor element has an affinity for at least two analytes and the plurality of nanotubes includes at least two types of nanotubes, a first type of nanotube having an affinity for a first analyte and a second type of nanotube having an affinity for a second analyte.
- the support structure includes a channel and the sensor element is suspended to span the channel.
- the support structure includes a conductive electrode positioned in the channel, and the sensor element is deflectable in response to the control circuitry to contact the electrode so that a semiconducting gating effect of the nanotubes in the sensor element may be electrically detected.
- an upper electrode is positioned above and separate from the sensor element.
- the sensor platform comprises a conductive element located apart from the sensor element so that the conductive element and the sensor element are in a capacitive relationship.
- circuitry to measure a capacitance associated with the conductive element and the sensor element comprises an addition ⁇ , reference capacitor that in turn comprises one or more nanotubes spaced apart from an additional conductive element.
- the sensor platform comprises a first conductive element contacting the sensor element at a first point and a second conductive element contacting the sensor element at a second point, so that an electric current can run through the sensor element between the first and second conductive elements.
- circuitry to measure the resistance between the first and second contacts to the sensor element comprises a reference resistor that in turn comprises one or more nanotubes separately contacted by conductive elements.
- a large-scale array of sensor platforms is provided in which the array includes a large plurality of sensor platform cells.
- a large-scale array of sensor platforms includes a plurality of sensor elements comprising one or more nanotubes
- sensors may be made by providing a support structure; providing one or more nanotubes on the support structure; and providing control circuitry to electrically sense the electrical characterization of the sensor element so that the presence of a selected analyte may be detected.
- the sensor element has an affinity for the selected analyte.
- the nanotubes are pristine nanotubes.
- the nanotubes are derivatized to have or to increase the affinity.
- the nanotubes are functionalized to have or to increase the affinity.
- a pattern is defined with respect to a collection of nanotubes on a support structure, which pattern corresponds to a .censor element; and a portion of the fabric is removed so that a patterned collection remains on the substrate to form the sensor element having a collection of at least one nanotube and having an electrical characterization.
- a collection of nanotubes is formed by growing the collection on the substrate using a catalyst.
- nanotubes are derivatized to have an affinity for a corresponding analyte.
- the nanotubes are functionalized to have an affinity for a corresponding analyte.
- the nanotube collection is formed by depositing a solution of suspended nanotubes on the substrate.
- the sensor elements are made of pre-derivatized nanotubes.
- the sensor elements are made of pre-functionalized n.anotubes.
- the nanotube collection is derivatized after its growth.
- the nanotube collection is functionalized after its growth.
- the patterned fabric remaining on the substrate is derivatized.
- the patterned fabric remaining on the substrate is functionalized.
- a conductive element located apart from the sensor element is provided so that the conductive element and the sensor element .are in a capacitive relationship.
- circuitry to measure a capacitance associated with the conductive element and the sensor element comprises an additional, reference capacitor that itself comprises one or more nanotubes spaced apart from an additional conductive element.
- a first conductive element and a second conductive element are provided such that the first conductive element contacts the sensor element at a first point and the second conductive element contacts the sensor element at a second point, so that an electric current can run through the sensor element between the first and second conductive elements.
- circuitry to measure the resistance between the first and second contacts to the sensor element is provided with a reference resistor that itself comprises one or more nanotubes separately contacted by conductive elements.
- a sensor element is substantially surrounded by support structure material so that it is not substantially exposed to contact with fluid that may contain an analyte, and thus may serve as a reference element.
- Figure 1 is a scanning electron micrograph showing a fabric of nanotubes conforming to the surface of a substrate such that a portion of the nanotube fabric is oriented substantially perpendicularly to a major surface of the substrate.
- Figures 2(A)-(E) illustrate nanotube fabric sensor devices according to certain embodiments of the invention;
- Figures 3(A)-(C) illustrate nanotube fabric sensor devices according to certain embodiments of the invention;
- Figures 4(A)-(L) illustrate acts of making vertical nanosensor devices according to certain embodiments of the invention;
- Figures 5-9 illustrate nanotube fabric sensor devices according to certain embodiments of the invention;
- Figures 10 and 11 illustrate hybrid technology embodiments of the invention in which nanosensor arrays use nanotube technology and standard addressing logic.
- Figures 12(A)-(B) .and 13 illustrate framed or patterned sensing-fabric structures and methods to create them.
- Figure 14 is a scanning electron micrograph of an array of contact holes, in each of which a sensor element could be located to form a large-scale sensor array.
- Preferred embodiments of the invention provide a new platform or vehicle to be used in sensors and sensor arrays for biological and/or chemical sensing. They can be built using conventional semiconductor fabrication techniques and can leverage existing manufacturing infrastructure and processes to create sensors employing carbon nanotubes. The manufacturing techniques are largely compatible with CMOS processes and can be conducted at lower temperatures than those for making prior-art nanotube sensing structures. They allow fabrication of a massive number of sensors on a given chip or wafer that can be integrated with various forms of control and computational circuitry.
- sensing elements are oriented substantially “vertically” - i.e., substantially perpendicular to the major surface of an associated substrate (which is understood to define the "horizontal” direction). Sensing elements may also be oriented "diagonally” - i.e., at orientations between the horizontal and vertical relative to the major surface of a substrate.
- nanofabrics elements made from a fabric of nanotubes
- These elements may be derivatized or functionalized as is taught in the art for individual nanotubes.
- these nanofabric elements provide a degree of redundancy (e.g., the sensor will still work even if a given tube in the element is faulty), are more easily manufactured, and may be manufactured as parts of l.arge arrays of sensors with complementary circuitry - for example, by locating sensor elements in each of a plurality of members of an array of contact holes like that pictured in Figure 14.
- the nanofabric elements may be either unmodified or functionalized so that they may be used to detect chemical analytes, such as organic and inorganic molecules.
- the chemical analyte may be a biological molecule such as peptides, proteins, or nucleic acids.
- the nanofabric may be functionalized, either non-covalently or cov.alently (e.g., by derivatization) so as to interact specifically with a particular analyte.
- the modified or unmodified analyte- sensitive nanofabrics may be incorporated into a nanosensor device for detection of the corresponding analyte in a sample.
- Preferred embodiments are understood to use the principle that charge tr.ansfer between SWNTs .and adsorbed molecules changes the nanotube conductance, so as to provide novel nanosensor schemes.
- Preferred embodiments provide methods and compositions for the detection of target analytes using changes in the conductivity of nanotube fabric upon binding of the analytes.
- Sensors according to certain embodiments of the present invention can be used in a way that allows detection and measurement of differences in their conductance or other electrical properties before and after the nanotubes are bound to analytes - e.g., by interacting non-covalently or covalently with a nanotube itself or with a complex consisting of a nanotube and a functionalization agent.
- the change in the sensor's electrical properties may be measured in conjunction with a gating electrode, disposed below or adjacent to the nanotubes, via a field effect on the semiconducting nanotubes, see, e.g., P. Qi et al., "Toward Large Arrays of Multiplex Functionalized Carbon Nanotube Sensors for Highly Sensitive and Selective Molecular Detection," Nano Lett, vol. 3, no. 3, pp. 347-51 (2003).
- a sensor with a suspended nanofabric structure.
- the change in the sensor's electrical properties may also be measured via an electromechanical mechanism in which differences between switching voltage with respect to, current through, or resistance of a nanofabric element in relation to an underlying electrode is determined before and after the nanofabric is exposed to analytes. Further, the physical presence of the sensed molecules or species may result in detectable strain on the suspended nanofabric, thereby potentially allowing molecular weight of the material to be determined directly. For example, as the strain energy changes due to binding of sensed molecules, a corresponding change in voltage could be measured.
- Nanosensors according to certain embodiments of the present invention are compatible with protocols that substantially prevent non-specific binding of non- target analytes.
- non-specific binding prevention see Star et al., “Electronic Detection of Specific Protein Binding Using Nanotube FET Devices," Nano Lett, vol. 3, no. 4, pp. 459-63 (2003).
- the nanofabric sensor of certain embodiments of the present invention may be used as an electrode in electrochemical sensors - for example, Clark-type sensors. See Lawrence et al., "A Thin-Layer Amperometric Sensor for Hydrogen Sulfide: The Use of Microelectrodes To Achieve a Membrane-Independent Response for Clark-Type Sensors," Anal. Chem., vol. 75, no. 9, pp. 2053-59 (2003).
- Figures 2(A)-(E) illustrate various embodiments of the invention.
- the sensor platforms may provide a vehicle in which a nanofabric element may be derivatized or functionalized after fabrication of the platform, but, in some embodiments, the derivatization or functionalization of the nanofabric element may be incorporated into the manufacturing steps of forming the sensor platform.
- an individual sensor cell is shown, but, as will be clear from the description below, the utilization of well-known semiconductor manufacturing techniques allows these individual sensor cells to be replicated on a massive scale so that a given chip or wafer may have a very large number of sensors that may be essentially identical to one another.
- the cells may be organized into massive arrays, small groups, or individual entities.
- the nanofabric element 202 of certain embodiments is formed from a non- woven fabric or layer of matted nanotubes (described in more detail below, and also described in incorporated references).
- the fabric is formed of single-walled carbon nanotubes (SWNTs), but other embodiments may utilize multi-walled carbon nanotubes (MWNTs) or mixtures of single- and multi- walled carbon nanotubes or other nanoscopic elements, such as nanowires.
- the fabric of certain embodiments is substanti ⁇ ly a monolayer of nanotubes with substantially constant porosity.
- This porosity may be substantially determined by, for e ⁇ .am ⁇ le, the number .and density of spin coats, which commonly also plays a principal role in substantially determining the capacitance of a particular nanofabric.
- the sensing parameters of the nanofabric element resemble those of individual nanotubes.
- the predicted sensing times and switching voltages for the nanofabric element should approximate the corresponding times and voltages for individual nanotubes.
- preferred embodiments of the present invention utilize fabrication techniques involving thin films and lithography. Such methods of fabrication lend themselves to generation of nanotubes and nanotube material over large surfaces, such as wafers 300mm in diameter.
- the nanofabric element should exhibit improved fault tolerances over individual nanotubes, by providing redundancy of conduction pathways through nanofabric elements. (If an individual nanotube breaks, other tubes within the fabric can provide conductive paths, whereas, if a sole nanotube were used and broken, the associated nanosensing cell would be faulty.) Moreover, the resistances of nanofabric elements should be significantly lower than those for individual nanotubes, thus decreasing their impedance, since a nanofabric element may be made to have larger cross-section.al areas than individual nanotubes.
- a monolayer fabric of single-walled nanotubes may be desirable, for certain applications it may be desirable to have multilayer fabrics to increase current density or redundancy, or to exploit other mechanical or electrical characteristics of a multilayer fabric. Additionally, for certain applications it may be desirable to use either a monolayer fabric or a multilayer fabric comprising multi- walled nanotubes or comprising a mixture of single-walled and multi-wdled n.anotubes.
- a n ⁇ tnosensor crossbar junction may be formed by a crossing of nanotubes and an electrode.
- Appropriate application of voltages to such a system can result in deflection of the nanotubes toward or away from the electrode, and, in certain embodiments, can result in a bistable junction with a pair of "on” or “off states - states in which the nanotubes are in stable positions of contact (e.g., electrical or physical) with the electrode or separation from the electrode, respectively.
- Figure 2(A) illustrates an exemplary platform (or sensor cell) 200 in cross-sectional view.
- Platform 200 includes a nanofabric element 202 that rests on or is pinned to supports 204 and 206. The element is suspended over an electrode 208 by a gap distance 210.
- FIG. 2(B)-(C) Two states of the nanofabric element 202 are shown with the perspective views of Figures 2(B)-(C).
- Figure 2(B) shows the platform in an undeflected state
- Figure 2(C) shows the platform in a deflected state in which the nanofabric element has been caused to deflect into contact with electrode 208.
- Switching between the states is accomplished by the application, or removal, of specific voltages across the nanofabric element 202 and one or more of its associated electrodes 208. Switching forces are based, in part, on the interplay of electrostatic attraction and repulsion between the nanofabric article 202 and the electrode 208.
- the second state of contact between nanofabric and electrode is "volatile”: e.g., the nanofabric moves into contact with the electrode only when voltage is applied, and returns to its undeflected state when the voltage is removed.
- the state of contact is "nonvolatile”: e.g., it may initially result from application of a voltage, but it continues after that voltage is removed.
- the electrode 208 may be used as a reference or as a field generator involved in measurement.
- a "reference" electrode could be used to prevent false positive or false negative readings by creating a comparison between a "sense" cell and a non-binding cell.
- each cell may be read by applying currents and/or voltages to nanofabric articles 202 and/or the electrode 208.
- the electrical properties of the sensor may then be measured (measuring apparatus is not shown).
- the nanofabric element 202 may contact the underlying electrode 208 and remain in contact, in a nonvolatile state.
- a change in the resistance or other electrical properties of the element 202, resulting from analyte binding - for example, a gating effect - may be detected. See P. Qi et al., "Toward Large Arrays of Multiplex Functionalized Carbon Nanotube Sensors for Highly Sensitive and Selective Molecular Detection," Nano Lett, vol. 3, no.
- the support structures 204 and 206 are made from silicon nitride (Si 3 N ) and are separated by about 180 nm. Meanwhile, the gap distance 202 is approximately 5-50 nm. Such a 5-50 nm gap distance is preferred for certain embodiments utilizing nanofabrics made from carbon nanotubes, and reflects the specific interplay between strain energy and adhesion energy for the deflected nanotubes. Gap distances of about 5-50 nm commonly create a platform in which a deflected state is retained in a nonvolatile manner, meaning the element 202 will stay deflected even if power is removed from the electrodes.
- the electrode 208 may be made of any suitable electrically conductive material and may be arranged in any of a variety of suitable geometries. Certain preferred embodiments utilize n-doped silicon to form such a conductive element, which can be, preferably, no wider than the nanofabric article 202, e.g., about 180 nm in width or less. Other embodiments utilize metal as conductor. In certain embodiments, the electrode 208 can be constructed from a nanofabric.
- the material of the support structures 204 and 206 may be made of a variety of materials and in various geometries, but certain preferred embodiments utilize insulating material, silicon nitride, or silicon oxide, and certain embodiments utilize electronic interconnects embedded within one support structure or both.
- the element 202 is held to the insulating support structures by friction.
- the nanofabric article 202 may be held by other means, such as by anchoring the nanofabric to the support structures using any of a variety of techniques. Evaporated or spin-coated material such as metals, semiconductors or insulators especially silicon, titanium, silicon oxide, or polyimide can be added to increase the pinning strength.
- the friction interaction can be increased through the use of chemical interactions, including covalent bonding through the use of carbon compounds such as pyrenes or other chemically reactive species.
- carbon compounds such as pyrenes or other chemically reactive species.
- R.J. Chen et al. "Non-covalent Sidewall Functionalization of Single- Walled Carbon Nanotubes for Protein Immobilization," J. Am. Chem. Soc, vol. 123, pp. 3838-39 (2001), and Dai et al., Appl. Phys. Lett, vol. 77, pp. 3015-17 (2000), for exemplary techniques for pinning and coating nanotubes by metals. See also WO 01/03208 for discussion of such techniques.
- the nanofabric article 202 may be coupled to another material by introducing a matrix material into the spaces between the nanotubes in a porous nanofabric to form a conducting composite junction, as described in the references incorporated above. Electrical and mechanical advantages may be obtained by using such composite junctions and connections.
- a conducting material is deposited onto the nanofabric and is allowed to penetrate into the spaces within the porous nanofabric, thus forming an improved electrical connection to the nanofabric and reducing the nanofabric article's contact resistance.
- an insulating material is deposited onto the nanofabric and is allowed to penetrate into the spaces within the porous nanofabric, thus forming an improved mechanical pinning contact that increases strain when the article is bent or deflected.
- Figure 2(C) illustrates a deflected nanofabric sensing switch according to one embodiment of the invention.
- the electrode or conductive trace 208 is disposed near enough to the suspended portion of the nanofabric element 202 that the two may contact one another when the nanofabric is deflected.
- the electrode 208 may also operate to create a field that can alter the electrical properties of a nearby nanofabric sensor; more particularly, the electrode 208 may create a field that alters the properties of semiconducting nanotubes in a nanosensor cell such as that of Figure 2(B). It is therefore an object of certain embodiments of the invention to create a nanofabric sensor composed substantially or entirely of semiconducting nanotubes disposed adjacent to a field-emitting electrode. See P.
- FIG. 2(D) illustrates another nanosensor cell 220.
- the electrode 208 of platform 200 is replaced with a nonmetal material 222 disposed adjacent to the suspended portion of the nanotube fabric 202.
- Pinning structures 224 are shown explicitly in this case. Such pinning structures can allow facile electrical connection to the nanofabric as well as providing support or clamping of the nanofabric to the underlying surface 204. Pinning structures would be conductive in many applications, but can be insulating or conductive, depending on the application.
- Figure 2(E) illustrates another nanosensor cell 226.
- the nanofabric element 202 is not suspended and instead rests upon support material 230.
- Support material 230 which may also be characterized as a pinning structure, may be anything consistent with use as a sensor, including but not limited to metals, alloys, ceramics, semiconductors, plastics, glass etc.
- Such a pinning structure can allow facile electrical connection to the nanofabric as well as providing support or clamping of the nanofabric to the underlying structure 204.
- a pinning structure would in many cases be conductive, but can be insulating or conductive, depending on the application.
- Figures 3(A)-(C) illustrate another sensor cell and the states such a cell might achieve.
- the nanofabric element 202 is positioned between a lower electrode 304 and upper electrode 306.
- the electrodes 304 and 306 (together with element 202) may be electrically stimulated to deflect the element 202 toward and away from electrode 304.
- the element 202 may be caused to deflect between the "at rest" state of figure 3(A) and the deflected state of figure 3(B).
- such a deflected state may be characterized as an "on" state in which the nanofabric-electrode junction is an electrically conducting, rectifying junction (e.g., Schottky or PN), which may be sensed as such through either the nanofabric article or the electrode 304, when addressed.
- the nanofabric article 202 may be deflected toward electrode 306 generating an "on" state different from the "on” state of the previous example (relevant electrical properties may be the same in both "on” states, but are addressed by different electrodes).
- FIG. 3(A)-(C) are not drawn to scale, and the gap distances 210 in a given cell, for example, need not be equal.
- the gap on one side of a nanofabric article 202 may be different from that on the other side, potentially to allow various combinations of volatile and nonvolatile switching behavior.
- inclusion of a third trace in the form of a release node can add a capacity to use this third trace to reset the cell or to isolate a particular cell. For example, a voltage could be applied to a third trace to isolate a cell by causing a nanofabric .article to be held in a particular nonvolatile state.
- each of the two conductive electrodes may be separately used to apply forces to move an electromechanically responsive nanofabric element, and each of the two conductive electrodes may serve as the "contact" for one of two alternative "on” states.
- the failure of one conductive trace may not be fatal to sensor junction performance.
- the structures as shown in Figure 3 generally facilitate packaging and distribution, and allow nanotube-technology cells to be more easily incorporated into other circuits and systems such as hybrid circuits.
- the nature of the electrical architecture can also facilitate the production of stackable sensor layers and the simplification of various interconnects. Techniques For Tailoring Characteristics Of Nanofabric Element
- Monolayer nanofabrics are made from single- or multi- walled nanotubes.
- the electrical properties of nanofabrics are highly tunable depending upon concentration of nanotubes within a given fabric. These characteristics can be controlled. For example, by selecting the proper length and width of a nanotube fabric as well as its porosity, a specific resistance per square can be measured in a range from 1-1000 kOhm/ ⁇ up to 1-10 megaOhm/D depending upon the type of device required and its necessary characteristics. Lower resistances may be achieved by shrinking the nanofabric dimensions and placing the nanofabric in contact with metal. Certain devices where the concentration of sensors must be higher might require a lower resistance nanofabric.
- a more sensitive device e.g., one that uses fewer nanotubes in the nanofabric
- Many specific methods of preparing the nanofabric can be envisioned, depending upon the specific sensing requirements for a particular device. Tuning methods of production, and the resulting products, to device requirements can be performed by using a combination of spin coating and photolithography in conjunction with functionalization or derivatization as described herein.
- Nanofabrics may be created by chemical vapor deposition (CVD) or by applying prefabricated nanotubes onto a substrate (e.g., spin coating).
- CVD chemical vapor deposition
- prefabricated nanotubes onto a substrate e.g., spin coating
- CVD-grown nanotubes are to be utilized, derivitazation or functionalization of the fabric are straightforward.
- a CVD-grown nanofabric can be derivatized or functionalized in the same fashion as the spin-coated fabric.
- Nanotubes grown by CVD can be doped during the growth process with a limited number of materials such as boron, silicon, indium, germanium, phosphorous, arsenic, oxygen, selenium, and other monatomic species using current technologies.
- CVD-grown nanotubes can be easily doped with an even wider variety of materials, including many types of molecules - for example, chemicals, drugs, DNA, RNA, peptides, or proteins.
- nanofabrics by spin coating pre-formed nanotubes is described in the incorporated and/or published patents and patent applications identified above. Such an approach has advantages over fabrication of nanofabrics by CVD. For example, lower temperatures may be used for manufacture of the device. This allows more materials to be used as a potential substrate in conjunction with the nanofabric element.
- prefabricated nanotubes may be derivatized or functionalized with nearly limitless agents before the nanotubes are applied to a substrate.
- Nanofabric sensors may be comprised of semiconducting nanotubes, metallic nanotubes or both. Investigators have shown that metallic nanotubes may be separated from semiconducting n.anotubes by precipitation. See, e.g., D. Chattopadhyay et al., "A Route for Bulk Separation of Semiconducting from Metallic Single- Walled Carbon Nanotubes," J. Amer. Chem. Soc, vol. 125, pp. 3370-75 (Feb. 22, 2003).
- nanofabrics of controlled composition semiconductor vs. metallic
- single- walled nanotubes are acid-treated and then functionalized non-covalently - e.g., in octadecylamine and tetrahydrofuran - causing metallic species to precipitate out of solution while leaving semiconducting nanotubes in solution.
- Either of the separate lots of nanotubes may be used for nanofabric creation once they are separated from one another.
- Separated nanotubes may be used to create nanofabrics for use as nanosensors with or without functionalization, and such nanotubes may be used in spin-coating applications and other appropriate methods as explained herein and in incorporated references.
- the relative concentrations of semiconducting and metallic nanotubes may be controlled. For example, one may create a fabric of approximately 90% semiconducting tubes and 10% metallic nanotubes by mixing a solution of 100% semiconducting nanotubes with a solution of unseparated nanotubes to acquire the desired concentration of each type of nanotube. Solutions of 100% semiconducting tubes may be mixed with solutions of 100% metallic nanotubes as well.
- Metallic nanotubes may also be destructively eliminated from already- formed nanofabrics by current-induced oxidation, see, e.g., P.G. Collins et al., "Engineering Carbon Nanotubes and Nanotube Circuits Using Electrical Breakdown," Science, vol. 292, pp. 706-09 (2001). It is an aspect of certain embodiments of the present invention to utilize the protocols set forth in this reference to create a nanofabric and to apply an appropriate voltage to it in order effectively to burn away metallic nanotubes. This method will work with nanofabrics that are created by CVD or by any other process, such as spin coating, etc.
- the nanofabric can be patterned by using standard lithography techniques, as described in the incorporated and published patent references.
- lithography techniques allow patterning of nanofabric by permitting the controlled definition of a region of fabric for use as a sensor element - for example, in the form of a nanotube ribbon of substantially predetermined dimensions.
- a nanosensor can be composed of carbon nanotubes or other highly robust materials, including nanowires, that can operate under extreme conditions with no loss of sensitivity.
- nanosensors Four general types of nanosensors have been envisioned: • pristine nanotubes (i.e., non-functionalized nanotubes) • non-covalently functionalized nanotubes • covalently derivatized nanotubes • a hybrid mixture of above. 1. Non-Functionalized, or Pristine, Nanotubes
- the first type of sensor utilizes pristine nanotubes in the nanofabric element - that is, the nanotubes are non-functionalized nanotubes.
- the surfaces of the nanotubes will adsorb analytes, which can alter electrical properties of the nanotubes, such as nanotube conductance or capacitance.
- nanotubes may adsorb molecules or species onto their surfaces, resulting in a measurable change in electrical characteristics, such as a change in conductivity, resistance, capacitance, etc.
- the change in electrical characteristic(s) may be measured directly from the nanotubes themselves via an appropriate electrical contact.
- Nanosensors can be used to detect concentrations of specific, known molecules. See L. Valentini et al., "Sensors for Sub-ppm NO 2 Gas Detection Based on Carbon Nanotube Thin Films," Appl. Phys. Lett, vol. 82, no. 6, pp. 961-63 (2003). It is therefore .an aspect of certain embodiments of the present invention to use nanofabric sensors to detect such concentrations.
- nanotubes Before nanotubes are applied to a surface to create a nanofabric, they can be functionalized in solution in order to increase the bonding of the tubes to a surface and/or to make possible the bonding of, or interaction with, analytes. It is therefore an object of certain embodiments of the present invention to functionalize individual nanotubes before they are used to create a nanofabric. It is a further object of certain embodiments of the present invention to use such functionalized nanotubes to create nanosensors, especially by patterning the nanofabric into specific shapes.
- Nanotubes may be functionalized in suspension before they are used to create a nanofabric, and such functionalized tubes may be stored in bulk before use.
- Such bulk-functionalized nanotubes may be mixed with pristine nanotubes to generate a partially functionalized nanofabric. More than one variety of functionalized nanotube solutions may be combined to generate mixtures of nanotubes to make mixed-functionalized nanofabrics. This procedure can be repeated to generate nanofabrics having as many different species of functionalized nanotubes as is desired for sensing. Thus, one could, for example, functionalize a nanotube solution with
- DNA sequences to sense from a test sample just particular species of interest such as those associated only with a specific virus or solely with specific forms of cancer.
- An aspect of certain embodiments of the present invention is the use of nanosensors in the detection of specific antigens or major histocompatibility complex (MHC)/antigen complexes from mixtures of fluids to be tested as an early warning sensor of disease or infection.
- MHC major histocompatibility complex
- nanotubes may be functionalized after nanotubes have been applied to a substrate in order to create a nanofabric.
- solution or gas phase functionalization could proceed before or after patterning the nanofabrics.
- This technique would lend itself to multiple spatially-addressable functionalization events across a surface. For example, one could envision using an inkjet-like process to spray various types of functionalizing agents onto specific regions of a substrate. Subsequent steps could be used to apply additional functional groups in the same or different regions to make nanosensor devices with regionally tailored sensing agents on the same substrate. In this way, many different types of analytes could be sensed by a given array, potentially with each cell sensing for the presence of a different analyte.
- nanotubes may be functionalized after sensing regions are patterned out of the bulk nanofabric.
- individual regions can be functionalized to serve as specific sensors.
- Multiple serial functionalizations or mixtures of functionalizing agents can be used to generate hybrid sensors capable of sensing more than one analyte at a time on a patterned nanofabric section or many such sections. This property lends itself to automation and use with robotics.
- Suitable analytes include organic and inorganic molecules, including biomolecules.
- the target analyte may be • any environmental pollutant(s), including pesticides, insecticides, toxins, etc.; • a chemical or chemicals, including solvents, polymers, organic materials, etc.; • one or more types of therapeutic molecules, including therapeutic and abused drugs, antibiotics, etc.; • one or more types of biomolecules, including hormones, cytokines, proteins, lipids, carbohydrates, cellular membrane antigens and receptors (neural, hormonal, nutrient, and cell surface receptors) or their ligands, etc; • whole cells, including prokaryotic (such as pathogenic bacteria) and eukaryotic cells, including mammalian tumor cells; • viruses, including retroviruses, herpes viruses, adenoviruses, lentiviruses, etc.; .and • spores; etc.
- any environmental pollutant(s) including pesticides, insecticides, toxins, etc.
- a chemical or chemicals including solvents, polymers, organic materials, etc
- potential analyte molecules include nucleic acids, oligonucleotides, nucleosides, .and their grammatical equivalents, as well as any and all modifications and analogs thereof, as understood in the art - including, for example, amino- or thio-modified nucleosides, and nucleotide molecules with alternate backbones or containing one or more carboxylic sugars, see, e.g., Beaucage et al., Tetrahedron, vol. 49, no. 10, p. 1925 (1993); Jenkins et al., Chem. Soc. Rev., pp. 169-176 (1995).
- molecules having at least two nucleotides covalently linked together could be potenti.al analytes.
- the category of potential analytes encompasses both single-stranded and double-stranded nucleic acids, as well as nucleic acids containing portions of both double-stranded and single-stranded sequences.
- a potential nucleic-acid analyte could be DNA (including genomic or cDNA), RNA, or a hybrid, where the nucleic acid contains any combination of deoxyribo- and ribo-nucleotides, and any combination of bases, including uracil, adenine, thymine, cytosine, guanine, inosine, xathanine, hypoxathanine, etc.
- Mimetic compounds for .any of the above might .also act as potential analytes.
- potential analytes include proteins, oligopeptides, peptides, and their analogs, including proteins containing non-naturally occurring amino acids and amino-acid analogs, and peptidomimetic structures.
- Any target analyte for which a binding ligand, described herein, may be made may be detected using the methods and articles of certain embodiments of the invention.
- Nanoimprint lithography may be used as a method of applying functionalization agents to discrete portions of nanofabric and thus to create discrete nanosensors. Such a method is primarily used for making massive arrays with sub- 100 nm features.
- Inkjet printing technology may be used for applying functionalization agents to discrete portions of a nanofabric to create separate nanosensors on a given wafer.
- Inkjet printing can be used to automate the functionalization of discrete nanosensor cells, either by applying functionalization agent to nanofabric cells directly, or by applying functionalized nanotubes to the area where a cell would reside on a substrate.
- Inkjet printing is a non-impact, dot-matrix printing technology in which droplets of ink or, in this case, nanotube solutions are "jetted" from a small aperture directly to a specified position on a surface or medium to create an image.
- a chemical etch procedure is performed to remove the gold nanocrystals and therefore also remove the avidin overlying the gold nanocrystals, leaving only the avidin attached to the ends of the nanotubes. It is therefore an aspect of certain embodiments of the present invention to fabricate nanosensors using this procedure and to immobilize protein at the ends of nanotubes used in nanosensing cells, articles, and elements.
- the sensors should be exposed to analytes, either as a part of a fully or nearly fully exposed system or as part of an encapsulated system whereby analytes are introduced in a controlled way.
- the nanofabric of a gas sensor may be fully exposed to the air
- the nanofabric of a DNA sensor might be encapsulated within a complex microfluidic analyte introduction mechanism.
- PCT publication WO 00/62931 "The Use of Microfluidic systems in the Electrochemical Detection of Target Analytes.”
- the inventors describe a sensor system whereby a fluid containing analytes is introduced to a sensing chamber by way of microchannels.
- Optional storage chambers and cell lysing chambers may be connected to the system by way of other microchannels. It is an object of certain embodiments of the present invention to utilize nanofabric sensors in such microfluidic systems.
- a detection surface comprises a detection electrode having a monolayer of conductive oligomers, and optionally a capture binding ligand capable of binding the target analyte.
- the target analyte directly or indirectly binds to the capture binding ligand to form a binding complex.
- the binding complex further comprises at least one electron transfer moiety. The presence of the electron transfer moiety is detected using the detection electrode. It is therefore an object of certain embodiments of the present invention to use the nanofabric sensor as the sensing element in the device according to the '839 patent to Kayyem.
- the nanosensor according to certain embodiments of the present invention may also be used as a detector according to the principles disclosed in U.S. Pat. No.
- Sheih relates to a microfluidic device with microchannels that have separated regions that have a member of a specific binding pair member such as
- Microchannels of embodiments of the invention are fabricated from plastic and are operatively associated with a fluid propelling component and detector.
- nanosensors according to certain embodiments of the present invention may also be used for analyte delivery and detection in conjunction with the nanofluidic channels described in incorporated references.
- the second type of sensor utilizes a nanofabric element in which nanotube surfaces are non-covalently functionalized. This allows for interaction with a wide variety of cations, anions, metal ions, small molecules, DNA, and proteins.
- Non-covalent functionalization takes advantage of non-covalent bonding of molecules to the sidewalls of nanotubes with substantial retention of the chemical structure and electrical characteristics of the nanotubes.
- Nanosensing devices can take advantage of such functionalization of nanotubes to increase, or make possible, bonding of nanotubes to analyte molecules or atoms.
- Nanofabrics may be non- covalently functionalized by adding pyrenes or other chemicals that are known to bind to nanotubes or graphite.
- 1-pyrenebutanoic acid and succinimidyl ester in organic solvent can be used to generate a succinimydyl functionalized nanotube.
- organic solvent such as dimethylformamide or methanol
- This method takes advantage of the pyrenyl group's interaction with the sidewalls of the nanotubes while generating succinyl ester groups that are highly reactive with nucleophilic substitution by primary and secondary amines found on the surfaces of most proteins and peptides as well as many drug and pro-drug compounds - where a "pro-drug" is, for example, an inactive precursor of a drug that is converted into active form in the body by normal metabolic processes.
- This functionalization mechanism is used to immobilize proteins and a wide variety of other biomolecules onto the sidewalls of SWNTs and to sense specifically for molecules that conjugate or bind those immobilized molecules preferentially.
- streptavidin may be adsorbed onto a nanotube surface in order to be used in immunohistochemical sensing. See Chen et al., "Non-covalent Sidewall Functionalization of Single walled Carbon Nanotubes for Protein Immobilization," J. Am. Chem. Soc., vol. 123, pp. 3838-39 (2001). The use of such nanosensors is compatible with analyte detection systems where non-specific binding is prevented.
- the third type of sensor utilizes a nanofabric element in which a covalently derivatized nanotube surface allows any of the interactions above.
- Nanotubes have been functionalized using covalent chemical bonding methods - e.g., involving diazonium salts. See J.L. Bahr et al., "Functionalization of
- Williams et al., supra uses an approach to providing covalently functionalized nanotube nanofabrics in which the unique properties of a nanofabric are combined with the specific molecule-recognition features of DNA by coupling a nanofabric to peptide nucleic acid (PNA, an uncharged DNA analogue) and hybridizing these macromolecular wires with complementary DNA.
- PNA peptide nucleic acid
- This allows the incorporating of DNA-derivatized nanofabrics into larger electronic devices by recognition-based assembly, and allows using nanofabrics as probes in biological systems by sequence-specific attachment.
- the technique used to couple nanofabrics covalently to PNA involves ultrasonically shortening nanofabric ropes for 1 hour in a 3:1 mixture of concentrated H 2 SO and HNO 3 .
- the PNA-derivatized nanofabric is transferred to water and dispersed in 0.5% aqueous sodium dodecyl sulphate.
- fragments of double- stranded DNA with 12-base-pair, single-stranded "sticky" ends that were complementary to the PNA sequence were used. These fragments were produced by cutting double-stranded DNA with restriction enzymes and ligating the products to single-str ⁇ mded oligonucleotides.
- This sticky DNA was hybridized to the PNA- nanofabric in water, deposited on freshly cleaved mica with 5 mM MgCl 2 . The surface was rinsed .and dried.
- Atomic-force micrographs of the DNA/PNA-nanofabric hybrids may then be recorded.
- the antisense properties of this derivatized complex may be exploited in biological applications, for example in biosensors.
- These methods allow appreciable and measurable functionalization of nanotubes with specific moieties or sensing agents added directly through covalent bonding.
- the functionalized nanotube becomes a reactive chemical itself and further chemistry can be performed to yield such diverse species as nanotubes with nanocrystals and inorganic compounds. See, e.g., S. Banerjee et al., "Functionalization of Carbon Nanotubes with a Metal-Containing Molecular Complex," Nano Lett., vol. 2, no. 1, pp.
- covalently functionalized nanotubes may be used in three ways to create nanosensors.
- the nanotubes may be functionalized separately and applied to a substrate, for example, by using a spin coating method or other method of application.
- the nanofabric may be applied to a substrate and subsequently covalently functionalized before patterning.
- the nanofabric may be functionalized after creation and patterning of the nanofabric.
- Each of these three methods lends itself to creation of a nanofabric comprising one or more types of functionalized nanotubes in the presence or absence of pristine nanotubes, depending upon the sensor application desired.
- a nanosensor can be fabricated using various methods.
- the fourth type of sensor uses a mixture of two or three of the previous types. By using such a mixture, a hybrid nanosensor is created with multiple binding- site types potentially able to detect multiple analytes and analyte types. Many different possible compositions of surface-functionalized nanotubes can be created before nanotubes are applied to the substrate, thereby allowing for a mixture of sensing components which can simultaneously screen for discrete analytes.
- Figures 4(A)-(L) collectively illustrate various intermediate structures created during an exemplary method for creating a substantially vertical nanosensor, including a nanosensor such as that of Figure 3(A). The steps shown are for illustrative purposes. Similar techniques and steps can be used to create other nanosensor structures, including those of Figures 2(D) and 2(E).
- a silicon wafer substrate 400 with an insulating or oxide layer 402 is provided. Alternatively, the substrate may be made from any material suitable for use with lithographic etching and electronics, and the oxide layer can be any suitable insulator. The oxide layer 402 is preferably a few nanometers in thickness, but could be as much as 1 ⁇ m thick.
- a second layer 404 is deposited on insulating layer 402.
- the second layer has a top surface 406.
- Two non-exclusive examples of the material from which the second layer 404 can be made are metal or semiconductor.
- a cavity 407 is defined in the second layer 404.
- the cavity 407 can be created in the second layer 404 by reactive ion etching, and is defined by inner walls 408 and, in certain embodiments, an exposed top surface 410 of insulating layer 402 at the base of the cavity. In certain other embodiments, a portion of second layer 404 remains such that the bottom of the cavity 407 is conductive.
- an insulating layer 412 could be provided to top surface 406 which could then be etched to generate a cavity.
- the cavity 407 can be prefabricated as part of a trench or a via provided as part of preprocessing steps - e.g., as part of an overall integration scheme in the generation of an electronic device.
- a first insulating layer 412 made of silicon nitride or other material is deposited on top of the exposed top surface 410 and top surface 406 to generate top layer 414 of intermediate structure 416 in Figure 4(B).
- the first insulating layer 412 is selectively etchable over polysilicon, nanotubes, silicon oxide, or another selected insulator.
- the first insulating layer 412 can act as a sacrificial layer to create a gap between subsequent layers and can be in a non-limiting range of thicknesses on the order of 100 to 200 nm.
- Nanotube fabric 418 is applied to intermediate structure 416, forming intermediate structure 420 of Figure 4(C).
- nanofabric layer 418 conforms to the underlying insulating layer 412 and substantially follows the geometry of cavity 407.
- the resulting structure 420 thus includes two vertical portions 418 A of the nanofabric 418, which portions are designed to be substantially perpendicular to a major surface of substrate 401.
- a second insulating layer 422 is applied over nanofabric 418.
- Protective insulating layer 424 which may be an oxide layer, is deposited on top of second insulating layer 422 having top surface 426, to form intermediate structure 428 of Figure 4(D). Deposition of protective insulating layer 424 on the sidewalls of the channel is substantially avoided.
- An exemplary but non-limiting thickness of protective insulating layer 424 can be on the order of 100 nm. The optimal thickness may be determined based on the need to protect the layers below protective layer 424 from additional etching or deposition steps.
- a non-exclusive example of the method of application of protective insulating layer 424 is sputtering or high-density plasma deposition of silicon dioxide.
- a polysilicon layer 430 is deposited on top surface 426 of intermediate structure 428 of Figure 4(D), filling the space between walls 408 in cavity 407 to give intermediate structure 432 of Figure 4(E).
- Polysilicon layer 430 can be deposited to a height greater than that of top surface 426 in order to get at least the proper amount of polysilicon layer into cavity 407, creating an overfilling condition as in intermediate structure 432.
- Polysilicon layer 430 may be subsequently planarized to etched polysilicon layer 434 with top surface 426 of oxide layer 424, as illustrated by intermediate structure 436 of Figure 4(F).
- Figure 4(G) illustrates etched polysilicon layer 434 etched to a first depth 438, by any appropriate method.
- An exemplary method of creating such a depth is by reactive ion etch ("RIE") and is shown in intermediate structure 440.
- First depth 438 later helps in the definition of one edge of a suspended nanofabric segment.
- the thickness of the etched polysilicon layer 434 depends, in part, on the depth of the original cavity 407, which, in certain embodiments, may be in a range from 200 nm to 1 micron. For certain applications requiring ultrahigh speed electromechanical switching sensors, this depth might preferably be below 200 nm. This depth can be reduced using thin film manufacturing techniques, as discussed below and in documents incorporated by reference.
- a layer of oxide 442 is deposited on exposed surfaces of intermediate structure 440 to form intermediate structure 448 of Figure 4(H).
- Vertical portions of oxide layer 446 cover trench walls, and horizontal portions of the oxide layer 444 cover top surfaces of polysilicon layer 434 and protective layer 424.
- Horizontal oxide layers 444 are removed - for example, by oxide spacer etching - leaving intermediate structure 450 of Figure 4(1).
- Figure 4(J) illustrates polysilicon layer 434 etched to a second depth 452.
- Second depth 452 may be approximately 50 nm deeper than first depth 438.
- the defined gap 454 allows exposure of regions of second insulating layer 422, as shown in intermediate structure 456.
- the regions 412A of first insulating layer 412 are removable - for example, by wet etching. Removal of materials from beneath a porous nanofabric has been described by the present applicants in incorporated references. Suitable wet etching conditions to remove regions of first insulating layer 412 and second insulating layer 422 leave a suspended nanofabric 458 having approximate vertical height 460 as observed in intermediate structure 462 of Figure 4(K). The wet etching may leave an overhang owing to the nature of isotropic wet etching conditions.
- Vertical height 460 is defined by the etching procedure. When vertical height 460 is about 200 nm, the thicknesses of first insulating layer 412 and second insulating layer 422 should preferably be approximately 20 nm if it is desired to have nanosensing elements have alternate nonvolatile "off and "on" states. If insulating layer thicknesses to generate an air gap are instead approximately 50 nm, deflected states may instead be volatile.
- Structure 462 of Figure 4(K) may be viewed as "final" structure incorporating two nanosensing elements like that shown in Figure 2(A).
- first insulating layer 412 had been made of a material not removed by the process that removed portions of second insulating 422, the structure that would have resulted would incorporate nanosensing elements like those of Figure 2(E).
- electrode material 466 may be deposited in trench 407, leaving gaps 468 between electrode material 466 and suspended nanotube fabric 458 as shown in intermediate structure 470.
- the resulting structure 470 has a pair of vertically suspended nanofabric portions 472 surrounded by vertical gaps 474 and 476 on either side of each vertically-suspended nanofabric portion 472.
- Structure 470 thus incorporates two nanosensing elements like that of Figure 3(A), and thus may serve as a basis for a pair of bi-state or tri-state switching sensors.
- Bi-state cells may be fabricated with the same elements as tri-state cells, but, in bi-state cells, the gap distance between the nanofabric and one electrode should preferably be great enough to prevent nonvolatile contact, but close enough to be used to switch off an oppositely disposed nonvolatile sensor cell.
- the behavior of such switching devices is influenced by the strain in the suspended nanofabric portions and the surrounding gap distances.
- structure 470 can be split into discrete “left” and “right” sections by a divide running vertically through electrode 466, leaving bi- or tri-state switches that may be independently operated.
- structure 470 can be split into discrete “left” and “right” sections by a divide running vertically through electrode 466, leaving bi- or tri-state switches that may be independently operated.
- the nature of the resulting devices and switches depends on the construction and arrangement of the electrodes and connections, among other factors. Attention is called to the construction of various types of electrodes in the following embodiments, as an indication of the flexibility of these devices and the variety of their potential uses.
- Some devices share common electrodes between more than one nanofabric article (e.g., two nanofabric switch elements being influenced by a same shared electrode). Other devices have separate electrodes that control the behavior of the nanofabric. One or more electrodes can be used with each nanofabric article to control the .article, as discussed, for example, in the incorporated reference entitled "Electromechanical Three-Trace Junction Devices.”
- FIG. 5 illustrates an exemplary structure with subsequent layers of metallization.
- This structure 500 includes electrode interconnect 502 and via 504 in contact with nanofabric 418, and a contiguous metallic layer 404 surrounding the electromechanical switch both laterally and subjacently.
- the nanofabric sensor is exposed to the milieu where it senses: although this may appear to be a closed structure, it is not necessarily so because areas surrounding the vertical nanosensor can be open to fluids of many types - for example, via open channels running through the three-dimensional structure (of which only a cross-section is shown in Figure 5).
- Figure 6 illustrates another exemplary structure with subsequent layers of metallization.
- This structure 600 is simile to intermediate structure 500 in several respects.
- an insulating layer 602 separates the portions of metallic layer 404, and therefore metallic layer 404 does not surround the electromechanical sensor elements, substantially preventing crosstalk.
- Figure 7 illustrates another exemplary structure with subsequent layers of metallization.
- Structure 700 differs from structure 600 in that the nanofabric layer 418 is not continuous, and there are thus two independent sensors 702 and 704, which have substantially no crosstalk.
- Figure 8 also shows an exemplary structure with subsequent layers of metallization.
- Structure 800 differs from structure 700 in that, instead of a single central electrode, there are two central electrodes 802 and 804 separated by insulating layer 806.
- Intermediate structure 800 has two nanosensors, which can be operated or read substantially independently.
- Figure 9 displays an additional exemplary structure with subsequent layers of metallization.
- Structure 900 is similar to intermediate structures 700 .and 800, except there is no central electrode at all.
- FIG. 3(A)-(C) show a device that has two distinct electrodes that can act together to push and/or pull a vertical nanofabric section. The gap distances help determine whether the devices are volatile or nonvolatile for a given set of parameters.
- Figures 6 and 7 show devices having three distinct electrodes and thereby providing extra degrees of freedom (e.g., extra redundancy, extra information storage or sensing capability, etc.).
- Figure 8 shows four distinct electrodes, since the center electrode is divided into two electrodes 802 and 804 by application of divider 806.
- Figure 9 shows two electrodes located on opposite sides of the channel, and uses top electrode 502 as a third electrode, one having a direct electrical connection to nanofabric section 418.
- Such a structure may be generated, in part, by using two standard photomasks to pattern gold contacts to a nanofabric line, which, for example, has dimensions of about 6 ⁇ m in length and 2 ⁇ m in width.
- the nanofabric contains pristine single-walled carbon nanotubes, and is treated with a mixture of 10 wt% polyethyleneglycol (PEG) with an average molecular weight of 25,000 and 10 wt% polyethyleneimine with an average molecular weight of 10,000 in water at room temperature overnight.
- PEG polyethyleneglycol
- the actual concentrations and amount of time required for this step can vary depending upon the size and density of the nanofabric required for the device. Also, it is noted that the nanotubes are exposed directly to solvent and must be handled with care in order to prevent damage to the nanofabric. For this reason, air drying rather than nitrogen blowing was performed. The nanotube fabrics could be allowed to dry in an oven with or without oxygen. After thorough rinsing in water, the nanofabric is subjected to a 15 mM solution of biotin-N-hydroxysuccinimide ester at room temperature overnight.
- the polymer- coated and biotinylated nanofabric can be tested for sensing capabilities by subjecting it to a 2.5 ⁇ M solution of streptavidin in 0.01 M phosphate buffered saline (pH 7.4) at room temperature. This test can be performed while electrical contacts are attached as long as the measurement voltage is sufficiently low. The electrical characteristics of the "pretested" (no streptavidin added) nanofabric are compared with those of the streptavidin-bound nanofabric to delineate a binding event.
- the total concentration of binding moieties can be determined by using streptavidin that is bound with gold particles.
- the particles for a given area of nanofabric can be counted by SEM or AFM to determine the order of magnitude sensitivity available within a particular device. Since such derivatization can take place over an entire wafer, it is easy to generate nanofabric sensors with a very narrow range of characteristic binding concentrations (over 4 orders of magnitude or more).
- the methods of fabrication for the nanotube sensors of certain embodiments of the present invention do not require the use of substrates that can withstand CVD temperatures. However, such substrates may also be used.
- the sensors of certain embodiments of the present invention are typically composed of nanotube fabrics that comprise redundant conducting nanotubes; these fabrics may be created via CVD, or by room-temperature operations as described herein and in incorporated references. In such a redundant sensor, if one sensing nanotube breaks, the device would remain operable because of the redundant conductive elements in each sensor. Because the nanosensor described herein can be fabricated at room temperature, the use of nearly any substrate, including highly flexible materials and plastics is possible.
- Nanosensors according to certain embodiments of the present invention can be readily manufactured using standard techniques found in the semiconductor industry such as spin coating and photolithography.
- the feature size of each nanosensor can be determined by photolithography or by deposition. Because such standard techniques are used in the construction of the nanosensors, the overall cost, yield, and array size can be larger than sensors created by other known techniques.
- N.anosensor cells according to certain embodiments of the present invention can be used in massive parallel arrays and can be multiplexed using standard CMOS- compatible sense amplifiers and control logic.
- the nanosensors according to certain embodiments of the present invention are compatible with high-resolution contact printing methods. See H. Li. et al., "High-resolution Printing with Dendrimers," Nano Lett, vol. 2, no. 4, pp. 347-49 (2002).
- Patterned nanofabrics may be created on a substrate (as described below and in incorporated references), and those patterned nanotubes may be transferred via an appropriate contact printing method to a second substrate. Par.ameters such as solubility and binding affinity are important factors to be considered in selecting suitable substrates.
- functionalized, patterned nanotubes may be transferred in the same manner.
- Nanosensors according to certain embodiments of the present invention can be produced on surfaces that can withstand CVD temperatures and also on surfaces that may not withstand such a harsh environment - e.g., when spin coating or aerosol application methods are used to create the nanofabric.
- the nanotubes of the nanofabric may be derivatized or functionalized prior to formation of the nanofabric, subsequent to the formation of the fabric, or subsequent to the patterning of the fabric.
- the three-dimensional structure might not be completely sealed but might instead have open channels whereby the nanofabric could be subjected to a derivatizing or functionalizing agent.
- the electrodes - for example, electrodes 466 and 404 of certain illustrated embodiments of the invention - may themselves be formed of nanofabric materials.
- having a nanofabric ribbon or other nanofabric article in place of a metallic electrode permits removal of sacrificial materials from regions beneath or next to the electrode. Fluid may flow through a nanofabric material disposed above or adjacent to a sacrificial layer to remove the sacrificial material.
- the devices and articles shown and described in the preceding embodiments are given for illustrative purposes only, and other techniques may be used to produce the same or equivalents thereof.
- the articles shown may be modified by the substitution of other types of materials or the use of different dimensions or geometries.
- some embodiments of the present invention may employ conductive interconnects made from, or comprising, nanotubes.
- using vertically oriented nanofabric articles permits exploitation of the smaller dimensions achievable with thin film technology, as opposed to those achievable with the lithographic techniques typically used for horizontally oriented nanofabric articles.
- the electrode 208 may be formed using thin film techniques, and the dimension T across which nanofabric may be suspended - in this case, essentially the same as the thickness of the electrode 208 - may be as little as a few nm thick (e.g., 10-100 nm, or less than 10 nm as technology develops). Gap distances such as distance 202 of Figure 2(A) can similarly scale downward with the development of thin film technology. Consequently, a vertically oriented nanofabric sensor created by thin film deposition can be much shorter in length than horizontally oriented nanofabric devices, such as those in incorporated references.
- a microfluidic delivery system may be utilized. Samples of blood, body fluids, chemicals, and the like may be injected or fed into a microfluidic delivery system. Such a system could then move material through a system of microfluidic capillaries and pumps to the sensor site. See, e.g., PCT publication WO 00/62931, "The Use of Microfluidic systems in the Electrochemical Detection of Target Andytes".
- Certain embodiments of the invention provide a hybrid technology circuit 1000, as shown in Figure 10.
- a core nanosensor cell array 1004 is constructed using nanofabric as outlined above, and that core is surrounded by semiconductor circuits forming X and Y address decoders 1006 and 1008, X and Y buffers 1010 and 1012, control logic 1014, and output buffer 1016.
- the control circuitry surrounding the nanosensing core may be used for conventional interfacing functions, including providing read currents and sensing output voltages at appropriate times. Other embodiments may include various forms of logic to analyze the outputs at appropriate times.
- the hybrid circuit 1000 may be formed by using a nanotube core (having either just nanosensor cells or nanosensor cells and addressing logic) and by implementing the surrounding circuitry using a field-programmable gate array.
- a gas input means 1102 is utilized in place of the microfluidic separator 1002, as shown in structure 1100 of Figure 11.
- Some of the advantages of the sensors according to certain embodiments of the present invention include an ability to implement large scale application and integration.
- one circuit chip may be used for the sensors and for processing of the information from the sensors and for control of the sensors. This is facilitated by having CMOS-compatible manufacturing processes.
- Figure 14 illustrates the possibilities for a large-scale array of addressable sensor elements by showing an array of contact holes in which sensor elements might be located.
- Certain embodiments provide methods for detecting changes in electrical properties such as nanosensor capacitance or resistance through use of a current mirror sensing approach, see, e.g., Baker et al., CMOS Circuit Design, Layout, and Simulation, pp. 427-33 (1998).
- investigators have shown that electrochemical properties of nanotube bundles and single carbon nanotube electrodes are reliable enough that such bundles and individual tubes can be used as electrodes in capacitors, see J.H. Chen et al., "Electrochemistry of Carbon Nanotubes and their Applications in Batteries and Supercapacitors," Electrochem. Soc, Proc, vol. 11, p. 362 (2001); Y.
- sensor cells may be constructed in which nanotube sensor elements are arranged in a capacitive relationship with one or more other conductive structures, and the structures and approaches to making such structures described therein can be readily extended to the vertically oriented sensors and methods for providing them described herein.
- material comprising nanotube fabric may be arranged so that it is on one side of an insulating layer (e.g., an Si 3 N 4 film), with a conductive pad being on the opposite side of the insulating layer.
- the nanotube-fabric material can act as one plate of a capacitor, the conductive pad can act as another plate, and the insulating layer can act as an intervening dielectric layer. Electrical connections and circuitry may then be provided to allow detection of the associated capacitance - for example, before and after exposure to a fluid (gas or liquid) that may carry a capacitance-altering analyte.
- the material comprising nanotube fabric might be protected from exposure by covering the side opposite the dielectric layer with a second insulating layer. The resulting capacitive structure could then be used to provide a reference capacitance, against which the capacitance of an analyte-sensitive capacitive structure could be measured.
- a sensor cell may be constructed so that an associated resistance may be measured, and the structures and approaches to making such structures described therein can be readily extended to the vertically oriented sensors and methods for providing them described herein.
- a resistance cell may be constructed, for example, by including electrical contacts at two or more different places on a nanofabric layer. Further electrical connections and circuitry may then be used to measure the resistance encountered when current runs through the nanofabric between two of the contacts.
- a "reference resistor” might be constructed by encapsulating the nanofabric within one or more protective insulating layers.
- the nanofabric cell could be exposed so that its measured resistance - and, more particularly, changes therein - might be an indicator of the presence or passage of an analyte or an analyte-carrying fluid.
- the fabric of a nanosensing capacitor may be made entirely of carbon nanotubes, or it may be made from nanowires of various composition - e.g., silicon nanowires - or the fabric may be a composite of nanotubes and nanowires.
- the creation of such nanowire and composite fabrics is more fully described in incorporated references such as U.S. provisional patent applications entitled "Patterning of Nanoscopic Articles.”
- Fluid samples delivered to a sensor element for analyte detection can include both liquids and gases, and may include analytes in a variety of forms - for example, as part of particulate matter suspended in a fluid.
- certain of the above aspects are applicable to individual nanotubes (e.g., using directed growth techniques, etc.) or to nanotube ribbons.
- phrases such as “collection of at least one nanotube” or “collection of one or more nanotubes” each generally encompass a number of one or more nanotubes, and potentially other matter, without regard to such considerations as whether any particular constituent or constituents of the collection have a special quality or distinctiveness, or are arranged in a particular way.
- a nanofabric sensor may be used as an electrode in a capacitor.
- Investigators have shown that electrochemic.al properties of n.anotube bundles .and single carbon nanotube electrodes are reliable enough that such bundles and individual tubes can be used as electrodes in capacitors. See J.H. Chen et al., "Electrochemistry of Carbon Nanotubes and their Applications in Batteries and Supercapacitors," Electrochem. Soc, Proc, vol. 11, p. 362 (2001); Y. Tu et al., “Nanoelectrode Arrays Based on Low Site Density Aligned Carbon Nanotubes," N ⁇ no Lett, vol. 3, no. 1, pp. 107-09 (2003). The present inventors have shown that electrical properties of single nanotubes are significantly maintained in nanofabrics (see incorporated references). It is therefore an object of certain embodiments of the present invention to use nanofabric as an electrode in a capacitor for use as a nanosensor.
- gaps of a porous nanofabric are especially helpful when capacitance differences are measured, because nanofabric/bound-analyte complexes exhibit different capacitances than the fabric sensor alone, and the capacitance difference is due in part to the greater surface are of the nanofabric alone, as opposed to the nanofabric with bound analytes.
- functionalization may in certain instances involve non-covalent transformation of the surface of a nanotube into a form with different function ⁇ groups or moieties, .and, for example, is meant to encompass any alteration or addition to a nanotube or nanotube surface - including covalent derivatization - that creates a product with different physical or electrical characteristics.
- Derivatization is indicative of a covalent alteration of the chemical structure of one or more nanotubes, or a portion thereof. In both circumstances, the process can be controlled such that electrical properties of nanotubes may be substantially retained.
- Functional groups can include inorganic atoms and molecules as well as organic molecules.
- Significant biological f nctional groups include peptides, nucleic acids, antigens (including polypeptide and non- polypeptide antigens) as well as peptide nucleic acids.
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Abstract
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EP1825038B1 (fr) | 2004-12-16 | 2012-09-12 | Nantero, Inc. | Liquide aqueux applicateurs de nanotubes de carbone et leur procede de production |
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2004
- 2004-05-12 EP EP04775994A patent/EP1631812A4/fr not_active Withdrawn
- 2004-05-12 WO PCT/US2004/014998 patent/WO2005019793A2/fr active Application Filing
- 2004-05-12 CA CA002526946A patent/CA2526946A1/fr not_active Abandoned
- 2004-05-12 US US10/844,883 patent/US7385266B2/en active Active
- 2004-05-12 WO PCT/US2004/014999 patent/WO2005031299A2/fr active Application Filing
- 2004-05-12 CA CA002525810A patent/CA2525810A1/fr not_active Abandoned
- 2004-05-12 US US10/844,913 patent/US7780918B2/en active Active
- 2004-05-12 EP EP04809372A patent/EP1623203A4/fr not_active Withdrawn
-
2006
- 2006-01-17 US US11/333,426 patent/US8310015B2/en not_active Expired - Lifetime
- 2006-01-17 US US11/333,623 patent/US7538400B2/en active Active
-
2007
- 2007-07-11 US US11/827,393 patent/US7786540B2/en active Active
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2009
- 2009-05-20 US US12/469,402 patent/US8357559B2/en active Active
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Cited By (20)
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US7670953B2 (en) | 2003-03-25 | 2010-03-02 | Molecular Imprints, Inc. | Positive tone bi-layer method |
US9099410B2 (en) | 2003-10-13 | 2015-08-04 | Joseph H. McCain | Microelectronic device with integrated energy source |
WO2006131400A1 (fr) * | 2005-06-10 | 2006-12-14 | Gilupi Gmbh | Nanocapteur de diagnostic et son utilisation en medecine |
US8846580B2 (en) | 2005-06-10 | 2014-09-30 | Gilupi Gmbh | Diagnostic nanosensor and its use in medicine |
US8197756B2 (en) | 2005-06-10 | 2012-06-12 | Gilupi Gmbh | Diagnostic-nanosensor and its use in medicine |
EP1896847A4 (fr) * | 2005-06-28 | 2011-12-07 | Korea Res Inst Chem Tech | Biocapteurs à base de transistor à nanotube de carbone avec des aptamères en tant qu'éléments de reconnaissance moléculaire et procédé pour détecter un matériau cible l'utilisant |
EP1896847A1 (fr) * | 2005-06-28 | 2008-03-12 | Korea Research Institute of Chemical Technology | Biocapteurs à base de transistor à nanotube de carbone avec des aptamères en tant qu'éléments de reconnaissance moléculaire et procédé pour détecter un matériau cible l'utilisant |
US7259102B2 (en) | 2005-09-30 | 2007-08-21 | Molecular Imprints, Inc. | Etching technique to planarize a multi-layer structure |
EP1811302A1 (fr) * | 2006-01-19 | 2007-07-25 | Topass Gmbh | Nano-capteur diagnostique et son usage |
WO2010034840A1 (fr) * | 2008-09-29 | 2010-04-01 | Commissariat A L'energie Atomique | Capteurs chimiques a base de nanotubes de carbone, procede de preparation et utilisations |
CN102203593A (zh) * | 2008-09-29 | 2011-09-28 | 法国原子能及替代能源委员会 | 含碳纳米管的化学传感器、其制备方法和其用途 |
FR2936604A1 (fr) * | 2008-09-29 | 2010-04-02 | Commissariat Energie Atomique | Capteurs chimiques a base de nanotubes de carbone, procede de preparation et utilisations |
US10106403B2 (en) | 2008-09-29 | 2018-10-23 | Commissariat à l'énergie atomique et aux énergies alternatives | Chemical sensors containing carbon nanotubes, method for making same, and uses therof |
CN101788516A (zh) * | 2010-02-22 | 2010-07-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | 交流电泳定向组装碳纳米管阵列传感器件的制作方法 |
EP2410767A1 (fr) * | 2010-07-22 | 2012-01-25 | Commissariat à l'Énergie Atomique et aux Énergies Alternatives | Capteur de pression dynamique mems, en particulier pour des applications à la réalisation de microphones |
FR2963099A1 (fr) * | 2010-07-22 | 2012-01-27 | Commissariat Energie Atomique | Capteur de pression dynamique mems, en particulier pour des applications a la realisation de microphones |
US8783113B2 (en) | 2010-07-22 | 2014-07-22 | Commissariat à{grave over ( )} l'énergie atomique et aux énergies alternatives | MEMS dynamic pressure sensor, in particular for applications to microphone production |
US8818007B2 (en) | 2010-07-22 | 2014-08-26 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | MEMS-type pressure pulse generator |
US10614966B2 (en) | 2014-08-11 | 2020-04-07 | Arizona Board Of Regents On Behalf Of The University Of Arizona | Aligned graphene-carbon nanotube porous carbon composite |
CN108375623A (zh) * | 2018-01-12 | 2018-08-07 | 宁波大学 | 基于快速扫描阳极溶出伏安技术检测食源性致病菌的电化学免疫传感器的制备方法及其应用 |
Also Published As
Publication number | Publication date |
---|---|
WO2005031299A8 (fr) | 2005-07-21 |
US7385266B2 (en) | 2008-06-10 |
EP1631812A2 (fr) | 2006-03-08 |
US7786540B2 (en) | 2010-08-31 |
WO2005031299A3 (fr) | 2009-04-09 |
EP1623203A2 (fr) | 2006-02-08 |
US8357559B2 (en) | 2013-01-22 |
US20080164541A1 (en) | 2008-07-10 |
US8310015B2 (en) | 2012-11-13 |
WO2005019793A2 (fr) | 2005-03-03 |
US20050053525A1 (en) | 2005-03-10 |
EP1623203A4 (fr) | 2010-11-24 |
US20100022045A1 (en) | 2010-01-28 |
WO2005019793A3 (fr) | 2008-10-30 |
US20050065741A1 (en) | 2005-03-24 |
CA2525810A1 (fr) | 2005-03-03 |
US7780918B2 (en) | 2010-08-24 |
US20060237805A1 (en) | 2006-10-26 |
US20060125033A1 (en) | 2006-06-15 |
EP1631812A4 (fr) | 2010-12-01 |
CA2526946A1 (fr) | 2005-04-07 |
US7538400B2 (en) | 2009-05-26 |
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